Hydrothermal synthesis and characterization of two new three-dimensional fluoroindium phosphates In4(PO4)4(H2O)4F2 • C6H14N2 and In8(PO4)8(H2O)8F4 • (C5H14N2)2

Two new three-dimensional fluoroindium phosphates, In-4(PO4)(4)(H2O)(4)F-2.C6H14N2 1 and In-9(PO4)(8)(H2O)(8)F-4.(C5H14N2)(2) 2, have been prepared under hydrothermal conditions by using triethylenediamine and 1-methylpiperazine as templates, respectively. They are characterized by inductively coupled plasma analysis, elemental analysis, fluoride ion-selective electrode, IR spectra and thermogravimetric analysis. The structures have been solved by single-crystal X-ray diffraction. Both the compounds crystallize in the monoclinic system, space group P2(1)/n (No. 14). Crystal data for 1, M = 1063.42, a = 10.3161(4) Angstrom, b = 12.7490(3) Angstrom, c = 17.9127(6) Angstrom, beta = 102.476(2)degrees, V = 2300.25(13) Angstrom(3), Z = 4. Crystal data for 2, M = 2102.80, a = 18.4673(6) Angstrom, b = 12.7117(5) Angstrom, c = 20.4705(7) Angstrom, beta = 108.566(2)degrees, V = 4555.4(3) Angstrom(3), Z = 4. They exhibit the same topological structure and are built up from vertex linking InO4(H2O)(2), InO4FH2O and InO4F2 octahedral and PO4 tetrahedral units, forming 6-membered ring channels along the a direction and two types of 8-membered ring channels along the b direction. The diprontonated triethylenediamine and 1-methylpiperazine molecules are entrapped in 8-membered ring channels. (C) 2004 Elsevier Inc. All rights reserved.